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WO2009057825A1 - Composition de résine de polypropylène, son procédé de fabrication, et article formé en mousse - Google Patents

Composition de résine de polypropylène, son procédé de fabrication, et article formé en mousse Download PDF

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Publication number
WO2009057825A1
WO2009057825A1 PCT/JP2008/070259 JP2008070259W WO2009057825A1 WO 2009057825 A1 WO2009057825 A1 WO 2009057825A1 JP 2008070259 W JP2008070259 W JP 2008070259W WO 2009057825 A1 WO2009057825 A1 WO 2009057825A1
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WIPO (PCT)
Prior art keywords
propylene
mass
ethylene
copolymer
resin composition
Prior art date
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PCT/JP2008/070259
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English (en)
Japanese (ja)
Inventor
Hiroyoshi Nakajima
Yoshitaka Kobayashi
Takashi Fujimoto
Original Assignee
Sumitomo Chemical Company, Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Chemical Company, Limited filed Critical Sumitomo Chemical Company, Limited
Priority to DE112008002889T priority Critical patent/DE112008002889T5/de
Priority to US12/739,896 priority patent/US8871825B2/en
Priority to CN200880113767.8A priority patent/CN101842436A/zh
Publication of WO2009057825A1 publication Critical patent/WO2009057825A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
    • C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers

Definitions

  • the present invention relates to a polypropylene resin composition, a method for producing the same, and a foam molded article.
  • Polypropylene is widely used in the molding field because it has excellent mechanical properties and chemical resistance and is extremely useful. Foam molded articles obtained by foaming polypropylene are used as cushioning materials, sound absorbing materials, water-permeable drain materials, various fillers and the like in the automotive field.
  • JP-A-10-87919 discloses (A) 50-95 parts by weight of polypropylene having a melt flow rate (ASTM D 12 38, 230 ° C, 2.16 kg load) of 10-100 g / 10 min. (B) 3 to 45 parts by weight of an amorphous or low crystalline ⁇ -year-old refin copolymer, and (C) 2 to 45 parts by weight of an inorganic filler (components (A), ( ⁇ ) and (C) (D) is a polypropylene resin composition obtained by melt blending 0.005 to 0.2 part by weight of an organic peroxide, and the polypropylene resin composition is (I) Melt flow rate (ASTM D 1 238, 230 ° C, 2.16 kg load) is 50 to 150 gZl O min.
  • the problem to be solved by the present invention is to provide a polypropylene resin composition and a method for producing the same, which can provide a foamed molded article with less silver streak. It is to provide a small amount of foamed molded body.
  • the present invention provides 0 to 70% by mass of a propylene homopolymer (A-1) and 30 to 100% by mass. / 0 of propylene one ethylene block copolymer of the following (A- 2) and including the propylene polymer (A), comprising ethylene one ⁇ - Orefin copolymer below (beta), and inorganic filler (C)
  • the ratio of the amount of ( ⁇ ) to the total amount of (A), ( ⁇ ) and (C) is 40 to 94% by mass, the proportion of the amount of ( ⁇ ) is 5 to 30% by mass, (C ) Is 1-30 mass ratio.
  • a polypropylene resin composition characterized by being / 0 .
  • Propylene-ethylene block copolymer ( ⁇ -2) A mixture of propylene homopolymer component and propylene-ethylene random copolymer component, 135 ° C tetralin of propylene-ethylene random copolymer component A mixture having an intrinsic viscosity measured in the range of 2.0 to 8.0 d 1 Zg;
  • a polypropylene-based resin composition obtained by heat-treating a premix having a mass percentage of 1 to 30 mass%.
  • the In this composition, the propylene / ethylene block copolymer ( ⁇ -2) and the ethylene / tetraolefin copolymer ( ⁇ ) are as defined in the composition according to the first aspect.
  • the present invention provides the method for producing a polypropylene-based resin composition according to the first aspect, wherein the propylene polymer (40) is 40 to 94 parts by mass, and the ethylene- ⁇ -olefin copolymer is First step of forming a preliminary mixture by supplying 5-30 parts by mass of coalescence (() and 5-30 parts by mass of the inorganic filler (C) to a melt-kneading apparatus (wherein (A), ( ⁇ ) And a total amount of (C) is adjusted to 100 parts by mass), and a second step of heat-treating the preliminary mixture by the melt-kneading apparatus. It is.
  • the present invention provides a polypropylene resin composition according to the first aspect. It is a foamed molded product characterized by Brief Description of Drawings
  • FIG. 1 is a schematic perspective view showing an example of the foamed molded product of the present invention produced in Examples.
  • Reference numeral 1 indicates an injection gate
  • reference numeral 2 indicates a range of a circle having a diameter of 6 Omm (part where silver streak was evaluated)
  • reference numeral 3 indicates a foamed molded body.
  • the polypropylene resin composition of this invention is 0-70 mass. /.
  • Propylene polymer (A) containing the following ethylene one alpha _ Orefu In-copolymer ( ⁇ ) and inorganic filler (C) are included, and the ratio of the amount of ( ⁇ ) to the total amount of (A), ( ⁇ ) and (C) is 40 to 94 mass. /.
  • the ratio of the amount of (ii) is 5 to 30% by mass, and the ratio of the amount of (C) is 1 to 30% by mass.
  • the propylene-ethylene block copolymer ( ⁇ -2) is a mixture of a propylene homopolymer component and a propylene-ethylene random copolymer component, and is a mixture of propylene-ethylene random copolymer components.
  • the ethylene- ⁇ -olefin copolymer (B) has a density of 0.85 to 0.89 g / cm 3 and is measured under a load of 1 90 ° C and 2.16 kg according to JISK 7210. Melt flow rate (hereinafter also referred to as “MFR”) is greater than 10 10 minutes and less than 40 g / ⁇ 0 minutes.
  • the polypropylene resin composition of the present invention is 0 to 70 mass. / 0 Propylene homopolymer (A - 1) and the propylene one ethylene block copolymer 30 to 100 mass 0/0 propylene polymer comprising (A- 2) containing (A).
  • the amount of (A_l) and the amount of (A-2) are ratios to the total amount of (A-1) and (A-2), respectively.
  • propylene polymer (A) examples include propylene homopolymer (A-1) and propylene monoethylene copolymer (A-2), propylene monoolefin copolymer, and propylene monoethylene mono ⁇ - You can also use olefin copolymer.
  • propylene mono- ⁇ -olefin copolymer examples include propylene mono ⁇ -Olefin random copolymer or propylene mono-olefin block copolymer.
  • the propylene mono ⁇ -olefin fin block copolymer is a mixture of a propylene homopolymer component and a propylene mono ⁇ -olefin fin random copolymer component.
  • propylene monoethylene ⁇ -olefin copolymer examples include propylene monoethylene _ ⁇ -olefin.
  • a random copolymer or a propylene monoethylene mono ⁇ -olefin block copolymer may be mentioned.
  • the propylene / ethylene / ⁇ -olefin block copolymer is a mixture of a propylene homopolymer component and a propylene / ethylene / ⁇ -olefin random copolymer component.
  • Examples of the ⁇ -olefin used in the propylene / ⁇ -olefin copolymer and the propylene / ethylene / ethylene copolymer include ⁇ -olefin having 4 to 20 carbon atoms, for example, 1-butene, 1_pentene, 1-hexene, 1-octene, 1-decene, etc.
  • the total amount of the propylene single child combination (A-1) and the propylene-ethylene block copolymer (2-2) occupy 50% by mass or more of the amount of the propylene polymer ( ⁇ ), and 80 mass. / It is more preferably accounts for 0 or more, 100 it is further preferable propylene homopolymer occupying mass% (A- 1) 1 3 C- Aisotakuchi' click as measured by NMR. Pentad fraction 0.95 or more More preferably, it is 0.98 or more.
  • Propylene one ethylene block copolymer of propylene homopolymer portion ( ⁇ _2), 1 3 C- NMR Aisotakuchikku 'pentad fraction, as measured by the lay preferred is 0.95 or more, more preferably is 0.98 or more .
  • the isotactic 'pentad fraction is the fraction of the propylene monomer unit at the center of the isotactic chain in the pentad unit in the propylene homopolymer molecular chain. This is the fraction of propylene monomer units in the linked chain (hereinafter referred to as mmmm).
  • the method of measuring the isotactic 'pentad fraction is determined by the method described by A. Zamb e 1 1 i et al. In Macro omo lecules, 6, 9 25 (1973), ie by 13 C-NMR. It is a method. The assignment of the NMR absorption peak is determined based on Macro 1 ecu 1 es, 8, 687 (1 975).
  • the ratio of the area of the mmmm peak to the area of the absorption peak in the methyl carbon region measured by 13 C-NMR spectrum is the ratio of the isotactic 'pentad fraction. It is. NP L reference material CRM No. M19-14 Polypropylene PP / MWD / 2 lysotactic 'pentad fraction of UK NAT I ONAL PHYS I CAL LA BORATORY measured by this method was 0.944.
  • Intrinsic viscosities measured in each are preferably from 0.6 to 5.
  • d 1 Zg Intrinsic viscosity of polymer (A-1) measured in 1 35 ° C tetralin solvent
  • Intrinsic viscosities measured in each are preferably from 0.6 to 5.
  • O d lZg more preferably from 0.7 to 4.0 dl / g, still more preferably from 0.8 to 2.0.
  • the propylene / ethylene block copolymer (A-2) contained in the propylene / ethylene block copolymer (A-2) was measured in a 135 ° C tetralin solvent.
  • the intrinsic viscosity (hereinafter also referred to as [77] EP ) is 2.0 to 8.0 dl / g, more preferably 2.5 to 6.0 dl / g.
  • the gel “permeation” of propylene homopolymer components of propylene homopolymer (A-1) and propylene monoethylene block copolymer (A-2) is used.
  • the molecular weight distribution measured by chromatography (GPC) (sometimes expressed as Q value or Mw / Mn) is preferably 3 to 7, respectively.
  • the ethylene content of the propylene-ethylene random copolymer component of the propylene-ethylene block copolymer (A-2) is preferably 20 to 65% by mass. More preferably 25-50 mass. / 0 , more preferably 30 to 45% by mass.
  • the content of the propylene monoethylene random copolymer component in the propylene monoethylene block copolymer (A-2) is 10 to 60% by mass, more preferably 10 to 40% by mass, and even more preferably 10 to 10%. 25% by mass.
  • the MFR of the propylene homopolymer (A-1) measured under a load of 230 ° C and 2.16 kg according to JIS K7210 is preferably 0.1 to 400 g / 10 min, more preferably Wow! ⁇ 300 g / 10 min.
  • the MFR of the propylene monoethylene block copolymer (A-2) measured under 230 ° C and 2.16 kg load according to JIS K7210 is preferably 0.1 to 200 gZl 0 min. Preferably it is 5 to 150 g / 10 minutes, more preferably 30 to; 1 30 gZ 10 minutes. From the viewpoint of foam moldability, the MFR of the propylene polymer (A) measured under 230 ° C and 2.16 kg load in accordance with JIS K7210 is preferably 0.1 to 200 g / l 0 Minutes, more preferably 5 to 150 g and 10 minutes.
  • the ratio of the amount of the propylene polymer ( ⁇ ) to the total amount of the propylene polymer (A), the ethylene- ⁇ -aged lefin copolymer ( ⁇ ) and the inorganic filler (C) 40-94 are mass%, it is laid more preferred is 40 to 80 wt%, Les more preferably it is 40 to 75 mass 0/0, the. If the content of the propylene polymer ( ⁇ ) is less than 40% by mass, the rigidity of the foamed molded product may be inferior. Further, if the content of the propylene polymer ( ⁇ ⁇ ⁇ ⁇ ⁇ ) exceeds 94% by mass, the impact resistance of the foamed molded product may be inferior.
  • the propylene homopolymer (A-1) and the propylene-ethylene block copolymer ( ⁇ -2) used as the propylene polymer ( ⁇ ) are produced by a known polymerization method using a known polymerization catalyst. can do.
  • the polymerization catalyst used in the production of the propylene polymer ( ⁇ ) include (1) a solid catalyst component containing magnesium, titanium, halogen and an electron donor as essential components, and (2) an organoaluminum compound. And (3) a catalyst system comprising an electron donor component.
  • This catalyst can be prepared, for example, by the methods described in Japanese Patent Application Laid-Open No. H11-31 9508, Japanese Patent Application Laid-Open No. 7-216017 and Japanese Patent Application Laid-Open No. 10-223119.
  • Examples of the polymerization method used in the production of the propylene homopolymer (A-1) and the propylene-ethylene block copolymer ( ⁇ -2) include the Barta polymerization method, the solution polymerization method, the slurry polymerization method, Examples include a phase polymerization method. These polymerization methods may be either batch type or continuous type, and these polymerization methods may be appropriately combined.
  • the method for producing the propylene / ethylene block copolymer ( ⁇ -2) is preferably a method using a polymerization apparatus in which at least two polymerization tanks are arranged in series, wherein the solid catalyst component (In the presence of the catalyst system comprising 1), an organoaluminum compound (2) and an electron donor component (3), a propylene homopolymer is produced by homopolymerizing propylene in a polymerization tank. The propylene homopolymer was transferred to the next polymerization tank, and propylene and ethylene were copolymerized in the polymerization tank in the presence of the propylene homopolymer. This is a method of forming a propylene-ethylene random copolymer component.
  • the amount of the solid catalyst component (1), the organoaluminum compound (2) and the electron donor component (3) used in the above method and the method of supplying each catalyst component to the polymerization tank may be determined as appropriate. ,.
  • the polymerization temperature is preferably from 1 ° to 300 ° C, more preferably from 20 ° to 180 ° C.
  • the polymerization pressure is preferably normal pressure to 1 OMPa, more preferably 0.2 to 5.0 MPa.
  • hydrogen may be used as the molecular weight modifier.
  • prepolymerization may be carried out before carrying out the main polymerization.
  • the prepolymerization method include a method in which a small amount of propylene is supplied in a slurry state using a solvent in the presence of the solid catalyst component (1) and the organoaluminum compound (2).
  • the polypropylene resin composition of the present invention includes an ethylene monoolefin copolymer ( ⁇ ), and the ethylene_ ⁇ -olefin copolymer ( ⁇ ) has a density of 0.85 to 0.89 gZ cm 3 .
  • Yes according to JIS K7210, measured at 190 ° C and under 2.16 kg load. Melt flow rate greater than 10 gZ for 10 minutes and 40 gZl for 0 minutes or less. It is a copolymer with olefin.
  • the polypropylene resin composition of the present invention may contain one type of ethylene-ct-olefin copolymer as the ethylene- ⁇ -olefin copolymer ( ⁇ ), or two or more types of ethylene.
  • One ⁇ -olefin copolymer may be contained.
  • ⁇ -Olefin used for ethylene- ⁇ -olefin copolymer ( ⁇ ) has 4 to 4 carbon atoms.
  • ⁇ -olefins such as 1-butene, 1_pentene, 1-hexene, 4-methyl-1-1-pentene, 1-heptene, 1-octene, 1-decene, 1-dodecene, 1-tetradecene 1 Monohexadecene, 1-eicosene and the like.
  • Olefin may be used alone or in combination of two or more. As hiefin
  • it is ⁇ -olefin having 4 to 12 carbon atoms such as 1-butene, 1-hexene, 1-octene and the like.
  • Ethylene mono ⁇ -olefin copolymer ( ⁇ ) is produced by polymerizing a predetermined monomer using a meta-octane catalyst by slurry polymerization, solution polymerization, bulk polymerization, gas phase polymerization, etc. can do.
  • metallocene catalyst examples include, for example, JP-A-3-163088 and JP-A-4-26.
  • the ethylene_ ⁇ -olefin copolymer ( ⁇ ) with respect to the total amount of the propylene polymer (A), the ethylene- ⁇ -olefin copolymer ( ⁇ ) and the inorganic filler (C)
  • the proportion of the amount is 5-30% by mass, preferably 10-30% by mass.
  • the content of ethylene- ⁇ -olefin copolymer ( ⁇ ) is 5 mass. /. If it is less than 1, the impact resistance of the foamed molded product may be inferior. Further, if the content of the ethylene / ⁇ -olefin copolymer ( ⁇ ) exceeds 30% by mass, the foam moldability may be inferior.
  • ethylene mono-olefin copolymer ( ⁇ ) 1 of the total amount of ethylene mono- ⁇ -olefin copolymer contained in the polypropylene resin composition is 30%. It preferably accounts for ⁇ 100% by weight, 50-100 mass. It is more preferable to occupy / 0 .
  • the ethylene content of the ethylene one alpha-Orefin copolymer (beta) is preferably 20 to 95 mass 0/0, more preferably from 30 to 90 wt%, alpha-Orefin content is preferably 80 5 mass 0/0, more preferably from 70 to 10 weight 0/0.
  • the density of the ethylene- ⁇ -olefin copolymer ( ⁇ ) is from 0.85 to 0.89 g / cm 3 , preferably from 0.85 to 0.88 g / cm 3 , and more preferably from 0.8. 86-0. is 88 g / cm 3. If the density is less than 0.85 g / cm 3 , foam moldability may be inferior. If it exceeds 0.89 gZcm, the uniformity and fineness of the foamed cells may be inferior. In addition, it is difficult to achieve good foam moldability and effective suppression of silver streak at the same time.
  • the melt flow rate measured under a load of 1 90 ° C and 2.16 kg is greater than 10 gZl 0 min, 4 O gZl O Min., Greater than 10 g / l 0 min, and preferably 35 gZl 0 min. If the melt flow rate is 10 gZl or less, silver streaks may occur in the foamed molded product.
  • the polypropylene resin composition of the present invention contains an inorganic filler (C).
  • the inorganic filler (C) is not limited, but specifically, granular fillers such as glass beads, carbonic acid ruthenium, and barium sulfate, kaolin, glass flakes, tanolec, layered catenate ( (Bentnite, montmorillonite, smectite), plate-like fillers such as My strength, fiber fillers such as fibers and whiskers, etc. Foam molded products with excellent flexural modulus by blending plate-like fillers Is obtained. Talc is inexpensive and preferred.
  • the average particle size of the inorganic filler (C) is preferably 0.01 to 50 m, more preferably 0.1 to 30 / im, and still more preferably 0.1 to 5 / xm.
  • the average particle size of the inorganic filler (C) is obtained from the integral distribution curve of the sieving method measured by suspending in a dispersion medium such as water or alcohol using a centrifugal sedimentation type particle size distribution measuring device. and it refers to a 50% equivalent particle diameter D 50.
  • Fibrous inorganic fillers are preferably used because of their excellent reinforcement performance.
  • the fibers used as the fibrous inorganic filler include glass fibers and metal fibers.
  • materials constituting the whisker used as fibrous inorganic filler include metals, inorganic compounds such as metal oxides and metal nitrides. Specifically, carbon, potassium titanate, sepiolite, wallastoni , Alofen, imogolite, magnesium oxysulfate, aluminum, nickel, copper, calcium carbonate, potassium aluminate titanate, titanium dioxide, calcium silicate, aluminum borate, magnesium borate, nickel borate, Examples include alumina and nitride nitride.
  • a whisker is preferred, and among them, a fibrous magnesium oxysulfate is preferred because the specific gravity of the fibrous filler itself is low and a molded product having excellent rigidity and appearance can be obtained.
  • a fibrous magnesium oxysulfate for example, Moshei (registered trademark) manufactured by Ube Materials Co., Ltd. may be mentioned.
  • the fibrous inorganic filler preferably has an average fiber length of 5 ⁇ m or more measured by electron microscope observation, more preferably 5 to 30 Atm, and even more preferably 10 to 20 ⁇ m. preferable. Further, the average fiber diameter is preferably 0.2 to 1.5 / im, more preferably 0.3 to 1.0 m.
  • the average aspect ratio of the fibrous inorganic filler is preferably 10 or more, more preferably 10 to 30, and even more preferably 12 to 25.
  • the average fiber diameter is 0.3 to 1.0 ⁇
  • the average fiber length is 7 to 15 ⁇
  • the average The aspect ratio is 12-25.
  • the average fiber diameter, average fiber length, and average aspect ratio of the fibrous inorganic filler were determined from images obtained by observation with a scanning electron microscope (SEM). It is obtained by selecting a filler, measuring its fiber diameter, fiber length, and aspect ratio and averaging.
  • the aspect ratio is the ratio of fiber length to fiber diameter.
  • the inorganic filler (C) may be used without treatment, and improves the interfacial adhesive strength with the polypropylene resin composition, or improves the dispersibility of the inorganic filler in the polypropylene resin composition. Therefore, the surface of the inorganic filler is treated with various known silane coupling agents, titanium coupling agents, higher fatty acids, higher fatty acid esters, higher fatty acid amides, higher fatty acid salts or other surfactants. Also good.
  • the inorganic filler (C) may be melt-kneaded with the propylene polymer (A) and Z or ethylene- ⁇ -olefin copolymer ( ⁇ ) in advance and used as a master batch.
  • the ratio of the amount of inorganic filler (C) to the total amount of propylene polymer ( ⁇ ), ethylene- ⁇ -olefin copolymer ( ⁇ ) and inorganic filler (C) Is 1-30 mass. / 0 , preferably 1 to 25% by mass, more preferably 1 to 20% by mass.
  • the content of inorganic filler (C) is 1 mass. If it is less than 0 , the foamed molded product may have poor rigidity. Further, if the content of the inorganic filler (C) exceeds 30% by mass, the impact resistance of the foamed molded product may be inferior.
  • the present invention in a second aspect, 0-7 0% by weight of propylene homopolymer (A- 1) Contact and 3 0-1 0 0 mass 0/0 Propylene one ethylene block copolymer (alpha-2 ) Containing a propylene polymer ( ⁇ ), ethylene- ⁇ -aged refin copolymer ( ⁇ ), and an inorganic filler (C), with respect to the total amount of (A), ( ⁇ ) and (C)
  • the proportion of the amount of ( ⁇ ) is 40 to 94% by mass, the proportion of the amount of ( ⁇ ) is 5 to 30% by mass, and the proportion of the amount of (C) is 1 to 30% by mass.
  • a polypropylene resin composition obtained by heat-treating a premix. In this composition, the definitions and details of the components (A-1), ( ⁇ -2), (A), ( ⁇ ) and (C) are the same as those in the composition according to the first aspect. is there.
  • the polypropylene resin composition according to the second aspect of the present invention comprises 2 parts by mass or less of an organic peroxide (100 parts by mass) with respect to 100 parts by mass of the total amount of (A), () and (C). It may be obtained by heat-treating a preliminary mixture further containing D).
  • the organic peroxide (D) can be selected from known organic peroxides. For example, an organic peroxide having a half-life of 1 minute and a decomposition temperature of less than 120 ° C, or a half-life Decomposition temperature at 1 min Mention may be made of organic peroxides having a temperature of 120 ° C or higher.
  • organic peroxides having a decomposition temperature of less than 120 ° C with a half-life of 1 minute include diacyl peroxide compounds and percarbonate compounds (represented by the following formula (1) in the molecular skeleton). And a compound (I) having a structure as described above and an alkyl perester compound (compound (II) having a structure represented by the following formula (2) in the molecular skeleton).
  • di (3-methoxybutyl) peroxydicarbonate di (2-ethylhexyl) peroxydicarbonate, bis (4 — T-butylcyclohexyl) peroxydicarbonate, diisopropyl baroxy dicarbonate, t-butyl peroxypropyl carbonate, dimyristyl carboxy carbonate and the like.
  • Compounds (II) having the structure represented by the above formula (2) include 1, 1, 3, 3-tetramethylbutyl neodecanoate, ⁇ -cumyl paroxyneodecanoate, t-butyl. Examples include peroxyneodecanoate.
  • organic peroxides having a decomposition temperature of 120 ° C or higher with a half-life of 1 minute include 1, 1-bis (t-butyl baroxy) cyclohexane, 2, 2-bis ( 4,4-di-mono-t-butylperoxycyclohexyl) Propane, 1,1-dibis (t-butyl carboxy) cyclododecane, t-hexyloxyisopropyl monocarbonate, t-butyl Ruperoxy-1,5,5-trimethylhexanoate, t-butylperoxylaurate, 2,5-dimethyl-1,2,5-di (benzoylperoxy) hexane, t-butylperoxyacetate, 2 , 2-bis (t-butylperoxy) butene, t-butylperoxybenzoate, n-butyl-1,4, bis (t-benoleoxy) glycolate, di-tert-butyl
  • the amount of the organic peroxide (D) used is preferably 2 parts by mass or less with respect to 100 parts by mass of the total amount of the above (A), (B), and (C).
  • the amount is more preferably 0.002 to 1 part by mass, and still more preferably 0.005 to 0.5 part by mass.
  • an embodiment in which a premix containing no organic peroxide (D) is heat-treated is also preferable.
  • the polypropylene resin composition of the present invention may contain an additive.
  • an additive include a neutralizing agent, an antioxidant, a light resistance agent, an ultraviolet absorber, a copper damage preventing agent, a lubricant, and a processing aid.
  • the melt flow rate measured under a load of 23 Q ° C and 2.16 kg in accordance with JIS K721 ⁇ of the polypropylene resin composition of the present invention is 50 to : 1 50 g / 10 min is preferable, and 50-: 120 gZl 2 O min is more preferable.
  • the MFR of the polypropylene resin composition is determined appropriately by determining the MFR of the propylene polymer (A) and the MFR of the propylene-ethylene block copolymer (B) used for the preparation of the composition. It can sometimes be adjusted by using an appropriate amount of organic oxide (D).
  • the polypropylene resin composition of the present invention comprises the propylene polymer (A) 40 to 94 parts by mass, the ethylene 1 ⁇ -olefin copolymer ( ⁇ ) 5 to 30 parts by mass, and the inorganic filler (C) 5 to A first step of supplying 30 parts by mass to a melt-kneading apparatus to form a preliminary mixture (however, the total amount of (A), ( ⁇ ) and (C) is adjusted to 100 parts by mass); It can be produced by a method including a second step of heat-treating the preparation mixture with the melt kneader.
  • organic peroxide (D) is further supplied to 100 parts by mass of the total amount of (A), ( ⁇ ) and (C).
  • the organic peroxide (D) is mixed with the propylene polymer (A), the ethylene monoolefin refin copolymer (B), and the inorganic filler (C) and simultaneously supplied to the melt-kneading apparatus. You may do it.
  • the heat treatment of the premix containing propylene polymer (A), ethylene alpha-alpha-refin copolymer ( ⁇ ⁇ ) and inorganic filler (C) is carried out by kneading each component with a melt kneader.
  • kneading apparatus used for kneading include a single screw extruder, a twin screw extruder, a knocker mixer, and a hot roll.
  • the kneading temperature is preferably 170 to 2500 ° C.
  • the kneading time is preferably 20 seconds to 20 minutes.
  • kneading may be performed after adding each component simultaneously, or may be performed while adding components sequentially. For example, it is preferable that a predetermined amount of each component is uniformly premixed with a tumbler or the like, and the resulting premix is melt-kneaded.
  • the foamed molded product of the present invention comprises the polypropylene resin composition of the present invention.
  • the foam molded article of the present invention can be obtained by foam molding the polypropylene resin composition of the present invention to which an appropriate amount of a foaming agent is added.
  • the foaming agent used in the present invention is not particularly limited, and known chemical foaming agents and physical foaming agents can be used.
  • the amount of the foaming agent added to the polypropylene resin composition to be subjected to foam molding is preferably 0.1 to 10 parts by mass, more preferably 0.1 to 100 parts by mass of the polypropylene resin composition. 2 to 8 parts by mass.
  • the chemical foaming agent may be an inorganic compound or an organic compound, and two or more compounds may be used in combination.
  • the inorganic compound include bicarbonates such as sodium bicarbonate.
  • the organic compound include polycarboxylic acids such as citrate and azo compounds such as azodicarbonamide (ADCA).
  • Examples of physical foaming agents include inert gases such as nitrogen and carbon dioxide, and volatile organic compounds. Among these, it is preferable to use supercritical carbon dioxide, nitrogen, or a mixture thereof. Two or more physical foaming agents may be used in combination, or chemical foaming agents and physical foaming agents may be used in combination.
  • a supercritical physical foaming agent has high solubility in the resin and can be uniformly diffused into the molten polypropylene resin composition in a short time. Therefore, the foaming ratio is high and foaming has a uniform foamed cell structure. A molded body can be obtained.
  • foam molding the polypropylene resin composition of the present invention include known methods such as injection foam molding, press foam molding, extrusion foam molding, and stampable foam molding.
  • the foamed molded article of the present invention can be made into a decorative foamed molded article by pasting a skin material by a method such as insert molding or adhesion.
  • the skin material a known skin material can be used.
  • the skin material include a woven fabric, a nonwoven fabric, a knitted fabric, a film made of a thermoplastic resin or a thermoplastic elastomer, a sheet, and the like.
  • a composite skin material in which sheets of polyurethane, rubber, thermoplastic elastomer, etc. are laminated on these skin materials may be used.
  • An additional cushion layer can be provided for the skin f age.
  • the material constituting the cushion layer include polyurethane foam, EVA (ethylene vinyl acetate copolymer) foam, polypropylene foam, polyethylene foam and the like.
  • Examples of uses of the foamed molded article of the present invention include automobile parts such as automobile interior parts and exterior parts, motorcycle parts, furniture and electrical parts, etc. Among them, automobile parts are preferable. More preferably, it is an interior part.
  • Examples of automotive interior parts include instrument panels, trims, door panels, side protectors, console boxes, and column covers.
  • automotive exterior parts include bumpers, fenders, and wheel covers.
  • Examples of motorcycle parts include a cowling and a muffler cover.
  • Intrinsic viscosity of the entire propylene-ethylene block copolymer [77] T 1.5 dl / g
  • Propylene monoethylene block copolymer (A-2) e-based talc masterbatch (C-2).
  • Predetermined amounts of each of the components shown in Table 1 were premixed uniformly with a tumbler, and the resulting premixed product was then mixed using a twin-screw kneading extruder (TEX44 SS 30BW-2V type, manufactured by Nippon Steel). , Kreu rotation speed 300 r pm, temperature 200 ° C, kneading under vent suction, resulting kneading The product was extruded at an extrusion rate of 30 to 50 kgZhr to produce a polypropylene resin composition pellet.
  • TEX44 SS 30BW-2V type manufactured by Nippon Steel
  • injection foam molding was carried out using an ES 2550/40 OHL-Mu C e 1 1 (clamping force 400 tons) manufactured by Engel. Nitrogen in a supercritical state was used as the blowing agent.
  • FIG. 1 For injection molding, a mold having a cavity having a shape corresponding to a molded body having a schematic dimension of 29 OmmX 37 OmmX 45 mm (height) is shown in FIG.
  • the basic cavity clearance (initial plate thickness) of the above-mentioned cavity in the clamped state was 1.5 mm (partially 1.6 mm), and the gate structure of the mold was a direct gate.
  • the cylinder temperature was set to 250 ° C and the mold temperature was set to 50 ° C.
  • injection of a polypropylene resin composition containing a foaming agent was started.
  • the cavity wall of the movable mold is moved backward by 2. Omm to increase the volume of the cavity, thereby increasing the volume of the polypropylene resin composition.
  • the foamed polypropylene resin composition was cooled and completely solidified to obtain a foamed molded product, and the state of the foamed molded product was evaluated at a site of 10 Omm from the injection gate. The results are shown in Table 1. .
  • the measurement was performed according to the method specified in JI S K7210. Unless otherwise specified, the measurement temperature was 230 ° C and the load was measured at 2.16 kg load according to the method specified in JISK7210.
  • Intrinsic viscosity of propylene-ethylene random copolymer component [ri] Inherent viscosity of propylene-ethylene random copolymer component of EP propylene-ethylene block copolymer [ ⁇ ] ⁇ is propylene alone Measure the intrinsic viscosity [] of the polymer component and the intrinsic viscosity [ ⁇ ] ⁇ of the entire propylene-ethylene block copolymer, respectively.
  • the mass ratio of the random copolymer component to the entire propylene / ethylene block copolymer: X was calculated from the following formula.
  • Mass ratio of propylene monoethylene random copolymer component to propylene monoethylene block copolymer as a whole X measures the heat of crystal fusion of the propylene homopolymer component and propylene monoethylene block copolymer as a whole, and uses the following formula: Was calculated. The amount of heat of crystal fusion was measured by suggestive scanning thermal analysis (DSC).
  • Ethylene content of propylene-ethylene random copolymer component of propylene-ethylene block copolymer (C2 ') EP is the ethylene content of the entire propylene-ethylene block copolymer by infrared absorption spectroscopy (C2') ⁇ was determined by calculation using the following equation. '
  • the measurement was performed according to the method specified in JISK 7 1 12. Measurements were made at 23 ° C using the water displacement method.
  • the flexural modulus of the polypropylene resin composition was measured according to the method specified in JISK 7 1 71.
  • a test piece molded by injection molding was used for the measurement.
  • the thickness of the test piece was 6.4 mm, and the flexural modulus was evaluated under the conditions of a span length of 10 O mm, a width of 12.7 mm, and a load speed of 2.0 mm / min.
  • the measurement temperature was 23 ° C.

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Abstract

Composition de résine de polypropylène caractérisée en ce qu'elle comprend un polymère de propylène (A) contenant de 0 à 70 % en masse d'un homopolymère de propylène (A-1) et de 30 à 100% en masse d'un copolymère bloc de propylène-éhylène (A-2) suivant, du copolymère d'éthylèneα-oléfine (B) suivant, et une charge inorganique (C), la quantité totale de (A), (B) et (C) étant comprise entre 40 et 94%, 5 à 30% et 1 à 30%, respectivement. Le copolymère bloc de propylène-éthylène (A-2) est un mélange d'un composant d'homopolymère de propylène et d'un copolymère aléatoire de propylène-éthylène dont la viscosité intrinsèque mesurée exprimée en tétraline à 135°C se situe entre 2,0 et 8,0 dl/g. Le copolymère d'éthylène-α-oléfine (B) est un copolymère d'éthylène et d'α-oléfine comptant de 4 à 20 atomes de carbone et ayant une densité de 0.85 à 0,89 g/cm3 et une fluidité à l'état fondu à 190°C sous une charge de 2,16kg selon JIS K 7210 supérieure à 10g/10 mn et de 40g/10 mn maximum.
PCT/JP2008/070259 2007-10-31 2008-10-30 Composition de résine de polypropylène, son procédé de fabrication, et article formé en mousse WO2009057825A1 (fr)

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US12/739,896 US8871825B2 (en) 2007-10-31 2008-10-30 Polypropylene resin composition, method for producing the same, and foam molded article
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